反应详情

2(S)-(tert-Butoxycarbonylamino)hexanoic acid (24.6 g, 0.106 mol), N,O-dimethylhydroxylamine hydrochloride (15.5 g, 0.15 mol), EDC hydrochloride (22.3 g, 0.117 mol) and HOBT (14.3 g, 0.106 mol) were stirred in dry, degassed DMF (300 mL) at 20° C. under nitrogen. N-Methylmorpholine was added to obtain pH 7. The reaction was stirred overnight, the DMF distilled under high vacuum, and the residue partitioned between ethyl acetate and 2% potassium hydrogen sulfate. The organic phase was washed with saturated sodium bicarbonate, water, and saturated brine, and dried with magnesium sulfate. The solvent was removed in vacuo to give the title compound.

1. customin dry
2. customdegassed DMF (300 mL) at 20° C. under nitrogen
3. additionN-Methylmorpholine was added
4. customto obtain pH 7
5. distillationthe DMF distilled under high vacuum
6. customthe residue partitioned between ethyl acetate and 2% potassium hydrogen sulfate
7. washThe organic phase was washed with saturated sodium bicarbonate, water, and saturated brine
8. dry with materialdried with magnesium sulfate
9. customThe solvent was removed in vacuo